Huagongshe화공사 화학 정보 인쇄 보고서 · 연구 참고용
Pyridine → 4-Methyl-N-(1,2,2,2-tetrachloroethyl)benzamide
참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|---|---|---|
| 반응물 | Pyridine | HCID 1049 | — |
| 반응물 | Diethyl Ether | HCID 3283 | — |
| 반응물 | Thionyl Chloride | HCID 24386 | — |
| 반응물 | 4-methyl-N-(2,2,2-trichloro-1-hydroxyethyl)benzamide | HCID 3392664 | — |
| 용매 | Dichloromethane | HCID 6344 | — |
| 생성물 | 4-Methyl-N-(1,2,2,2-tetrachloroethyl)benzamide | HCID 12341576 | 89.2% |
반응 단계
A stirred solution of Example 37C (20.0 g, 70.8 mmol) in CH2Cl2(300 mL) at 0° C. was treated with pyridine (10 mL). The reaction mixture was treated dropwise with thionyl chloride (10.4 mL, 141 mmol), and the reaction flask was equipped with a calcium chloride drying tube. The reaction mixture was warmed to ambient temperature and stirred for 4 hours. Concentration of the reaction mixture to a reduced volume and addition of diethyl ether (100 mL) resulted in a precipitate which was filtered off, and the filtrate was concentrated and dried under reduced pressure to provide 19.0 g of the desired product as a white solid.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 특허 번호 | US06645968B2 |
| 출처 데이터셋 | uspto-grants-2003_11 |
| ORD ID | ord-3714a12322254811b07426d335532996 |
| 출처 메모 | uspto-grants-2003_11 |